Detection of Avanafil and Flibanserin in Health Food by HPLC-MS/MS / 医药导报

Objective To develop a method for detection of avanafil and flibanserin adulterated in health food by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods The separation and analysis were performed on an Agilent Eclipse Plus C18 column(2.1 mm×100 mm,1.8 μm),with a mobile phase of acetonitrile and 0.1%acetic acid(containing 20 mmol·L-1 ammonium acetate)(60:40).Electrospray ionization(ESI) source was applied and operated in positive mode.Multiple reaction monitoring(MRM) mode was used to quantify avanafil and flibanserin.Results The assay linearity of avanafil and flibanserin were confirmed in the range of 2-20 ng·mL-1(r2>0.99).The extraction recoveries varied from 94.6% to 110.0%,and the precision of RSD was <5.0%.The limits of detection were 0.21 and 0.42 μg·kg-1 for avanafil and flibanserin,respectively.Conclusion The method was specific,sensitive and accurate.Therefore,it can be used to detect avanafil and flibanserin which were illegally added in health food.

Quality Standard of Xiao'er Resuqing Granules / 医药导报

Objective To establish the quality standard of Xiao'er resuqing gantules.Methods Rhei Radix et Rhizoma,Bupleuri Radix,Forsythiae Fructus,Puerariae Lobatae Radix in the granules were qualitatively identified by the method of thin layer chromatography (TLC).The content of baicalin was analyzed by the method of high performance liquid chromatography (HPLC).Results There were good specificities of the TLC method to identify Rhei Radix et Rhizoma,Bupleuri Radix,Forsythiae Fructus,Puerariae Lobatae Radix.The linear range of baicalin was 0.116 2-1.743 0 μg (r =1.000 0).The average of recovery and RSD were 100.61％,0.79％ (n =6),respectively.Conclusion The method established in this study is simple,accurate,reliable and suitable to be applied to quality control for the preparation of Xiao' er resuqing granules.

Determination of 7-ethyl-10-hydroxycamptothecin in microdialysates from rat brain with LC-MS/MS / 浙江大学学报·医学版

<p><b>OBJECTIVE</b>To establish a method for determination of 7-ethyl-10-hydroxycamptothecin (SN-38) in microdialysates from rat brain.</p><p><b>METHODS</b>The concentrations of SN-38 were measured by LC-MS/MS method with Agilent Eclipse Plus C18 (2.1 mm ×100 mm, 1.8 μm) reversed phase column using acetonitrile-0.1% methanoic acid as mobile phase with gradient elution at a flow rate of 0.3 ml/min and temperature at 35 degree. Multiple reaction monitoring using the precursor to product ion combinations of m/z 393.1→349.1 was performed to detect SN-38 in microdialysates from rat brain.</p><p><b>RESULTS</b>Blank microdialysate had non-interference. The method was linear over the concentration range of 0.1015-1015 ng/ml (r=0.9995); and the lower limit of quantification (LOQ) was 0.1015 ng/ml. The recovery of assay for SN-38 ranged from 97.54%-100.60%. The intra- and inter-day precision and stability were both well. The concentrations of SN-38 in brain microdialysates presented pharmacokinetics process and achieved the peak after 220 min.</p><p><b>CONCLUSION</b>The fully validated LC-MS/MS analytical method has high specificity and sensibility, which can be used effectively to analyze SN-38 in microdialysates from rat brain.</p>

Preparation of ligustrazine-chitosan microspheres by spray drying method / 中草药

Objective To prepare ligustrazine-chitosan microspheres and to investigate the drug release behavior in vitro. Methods Microspheres were prepared using the spray drying method.The encapsulation efficiency was used to evaluate the influence of different formulation and preparation factors,the formulation was optimized by L9(34) orthogonal design.Results The optimal formulation and preparation factors were as follows: chitosan concentration(0.01 g/mL),ratio of chitosan to ligustrazine(1∶4),inlet temperature(120 ℃),air flow rate(500 L/h).The optimized microspheres had a spherical shape,the loading capacity was(18.60?0.15)%,entrapment efficiency was(93.01?0.76)%,the average diameter was(10.69?0.64) ?m.The drug release profile in vitro could be described by Higuchi equation Q=19.798 t1/2+25.209(r=0.997) at 1-15 h,which showed the prepared microspheres obviously had the sustained release effect.Conclusion The encapsulation efficiency of ligustrazine-chitosan microspheres is higher,the preparation method is simple,and the process is stable.It will provide the basis for realizing the industrialization in Chinese materia medica microspheres.